1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid and preparation method thereof

A technology of methyl imidazole tetrafluoroborate and propanol tetrafluoroborate, which is applied in 1 field and achieves the effects of convenient operation, good thermal stability and low vapor pressure

Inactive Publication Date: 2010-06-30
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report about 1,3-bis-(1-methy

Method used

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  • 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid and preparation method thereof
  • 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid and preparation method thereof
  • 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Synthesis of 1-(3-chloro-2-hydroxy-propyl)-3-alkylimidazolium tetrafluoroborate ionic liquid

[0026] Dissolve 20mL of 1-methylimidazole (10.3g, 0.25mol) in 50mL of ethanol, add 33.20mL of tetrafluoroboric acid (0.25mol, 48% aqueous solution) in batches under stirring at 0°C, and react for 60 minutes under the same conditions after the addition 19.6 mL of 3-chloro-propylene oxide (23.12 g, 0.25 mol) was added dropwise to the reaction solution under stirring condition. After the drying tube was equipped, the reaction bottle was placed in the water bath of the experimental ultrasonic cleaner, and reacted with ultrasonic radiation (power 300W, frequency 40KHz) at 20°C for 3h, and TLC detected that the reactant disappeared. The solvent was removed by rotary evaporation under reduced pressure at 60°C, and the colorless liquid was 51.18g of 1-(3-chloro-2-hydroxy-propyl)-3-methylimidazolium tetrafluoroborate ionic liquid after vacuum drying at 80°C for 12 hours , the yiel...

Embodiment 2

[0030] (1) Synthesis of 1-(3-chloro-2-hydroxy-propyl)-3-alkylimidazolium tetrafluoroborate ionic liquid

[0031] Dissolve 20mL of 1-methylimidazole (10.3g, 0.25mol) in 50mL of ethanol, add 33.20mL of tetrafluoroboric acid (0.25mol, 48% aqueous solution) in batches under stirring at 0°C, and react for 60 minutes under the same conditions after the addition 19.6 mL of 3-chloro-propylene oxide (23.12 g, 0.25 mol) was added dropwise to the reaction solution under stirring condition. After the drying tube was equipped, the reaction bottle was placed in the water bath of the ultrasonic cleaner used in the experiment, and reacted with ultrasonic radiation (power 300W, frequency 40KHz) at 30°C for 4h, and the reactant disappeared as detected by TLC. The solvent was removed by rotary evaporation under reduced pressure at 60°C, and the colorless liquid was 53.06g of 1-(3-chloro-2-hydroxy-propyl)-3-methylimidazolium tetrafluoroborate ionic liquid after vacuum drying at 80°C for 12 hours ...

Embodiment 3

[0035] (1) Synthesis of 1-(3-chloro-2-hydroxy-propyl)-3-alkylimidazolium tetrafluoroborate ionic liquid

[0036] Dissolve 20mL of 1-methylimidazole (10.3g, 0.25mol) in 50mL of ethanol, add 33.20mL of tetrafluoroboric acid (0.25mol, 48% aqueous solution) in batches under stirring at 0°C, and react for 60 minutes under the same conditions after the addition 19.6 mL of 3-chloro-propylene oxide (23.12 g, 0.25 mol) was added dropwise to the reaction solution under stirring condition. After the drying tube was equipped, the reaction bottle was placed in the water bath of the ultrasonic cleaner used in the experiment, and reacted under ultrasonic radiation (power 300W, frequency 40KHz) at 40°C for 6h, and the reactant disappeared as detected by TLC. The solvent was removed by rotary evaporation under reduced pressure at 60°C, and the colorless liquid was 55.68g of 1-(3-chloro-2-hydroxy-propyl)-3-methylimidazolium tetrafluoroborate ionic liquid after vacuum drying at 80°C for 12 hours...

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Abstract

The invention discloses ion liquid containing symmetrical functional groups, in particular to 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid and a preparation method thereof. The 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid has a general structure formula as follows. The preparation method of the 1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid comprises the following steps of: dissolving 1-methylimidazole into 2-3 times of alcohol; adding tetrafluoroboric acid with 0.9-1.1 times of molar weight under ice-water bath stirring at -5-10 DEG C; reacting for 30-90 minutes under the same condition, and then dripping 3-chlorine-propylene oxide with 0.8-1.0 times of molar weight to a reaction bulb; after a drying tube is prepared, placing the reaction bulb in a water bath of an experimental ultrasonic cleaner, and ultrasonically radiating (with the power of 300 W and the frequency of 40 KHz) and reacting for 3-12 hours under the condition of 15-70 DEG C; removing a solvent through rotation, decompression and evaporation; drying for 12 hours in vacuum at 80 DEG C and then obtaining an intermediate compound; then mixing the intermediate compound with the 1-methylimidazole with the molar ratio of 1:1.2-1:2.5; adding absolute alcohol with 2-3 times mount of total amount; then adding the tetrafluoroboric acid with 1.2-1.5 times of molar weight; reacting for 2-8 hours under the stirring condition at -5-10 DEG C; then increasing temperature to 10-60 DEG C, and reacting for 12-24 hours; removing the solvent through the rotation, the decompression and the evaporation; and drying for 12 hours in vacuum at 80 DEG C and then obtaining the pure1, 3-di-(1-methylimidazole)-2-propanol tetrafluoroborate ion liquid.

Description

Technical field: [0001] The invention belongs to the technical field of chemical material synthesis, relates to an ionic liquid containing symmetrical functional groups, in particular to a 1,3-bis-(1-methylimidazolyl)-2-propanol tetrafluoroborate ionic liquid and its synthesis method. Background technique: [0002] Due to almost no vapor pressure, high chemical and thermal stability, wide electrochemical window, ionic liquids have good solubility for inorganic substances, organic substances, catalysts and polymers, and can be adjusted by designing the cationic part of the ionic liquid Its performance has become the widespread concern of scholars at home and abroad. At present, the research interest in ionic liquids is showing an unprecedented surge trend, and a large number of articles and patents related to the application of ionic liquids in organic synthesis and catalytic chemistry, biotechnology, electrochemistry and materials chemistry have been published (Deetlefs M, ...

Claims

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Application Information

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IPC IPC(8): C07D233/60
Inventor 詹天荣侯万国徐洁
Owner QINGDAO UNIV OF SCI & TECH
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